Phase-selective staining of metal salt for scanning electron microscopy imaging of block copolymer film

Li, Jingze; Wang, Ying; Wang, Zhi Hong; Mei, Di; Zou, Wei; Chang, Ai Min; Wang, Qi; Komura, Motonori; Ito, Kaori; Iyoda, Tomokazu

doi:10.1016/j.ultramic.2010.06.006

Cited by 9 publications

(7 citation statements)

References 28 publications

(52 reference statements)

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“…The mean diameter of the PEO cylinders is around 22 nm, and the average spacing of cylinder to cylinder is around 38 nm. However, no contrast was presented by SEM, as shown in figure 2(c), agreeing with the general knowledge that a staining process is required prior to SEM imaging of an electrical insulator [27]. After treating the BCP film with HAuCl 4 solution, there is no obvious change in the surface morphology as discovered by AFM height-mode and phasemode images (figures 2(d) and (e)).…”

Section: Resultssupporting

confidence: 80%

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Solvent induced formation of an ordered nanorod array of gold/polymer composite by block copolymer film templating

Zou¹,

Wang²,

Wang³

et al. 2011

Nanotechnology

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We report a novel method to fabricate ordered arrays of gold-polymer composite nanorods with the orientation in the vertical direction using block copolymer (BCP) film. The salt precursor is selectively infiltrated within vertically aligned cylindrical domains of the BCP film by immersing the template in a simple aqueous solution of HAuCl(4). Scanning electron microscopy suggests that the salt might be uniformly positioned along the polymeric cylinders. A subsequent vacuum ultraviolet light irradiation simultaneously reduces the HAuCl(4) into spherical gold nanoparticles with mean diameter around 2 nm and removes the matrix of the BCP template to produce metal-polymer composite nanorods. While the solvent is methanol, the salt might be concentrated at the bottom of the BCP film. As a result, a periodic pattern of gold nanoparticles with average diameter around 11 nm is formed where the BCP film is completely etched away. The solvent can effectively tune the spatial distribution of the salt precursor along the polymeric cylinders, which is responsible for the different morphologies of the photochemically fabricated nanostructures.

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Section: Resultssupporting

confidence: 80%

“…In contrast, for the aqueous solution treated sample, the salt may be homogeneously distributed along the PEO cylinder. This is the reason why a phase contrasted pattern can be visualized by SEM imaging [27]. It is well known that the evaporation speed of methanol is much faster than that of water.…”

Section: Resultsmentioning

confidence: 99%

Solvent induced formation of an ordered nanorod array of gold/polymer composite by block copolymer film templating

Zou¹,

Wang²,

Wang³

et al. 2011

Nanotechnology

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“…There is only one report on utilizing metal salts such as silver nitrate and chloroauric acid as a staining reagent. However, that method had multiple steps and required a time intensive photoreduction . To our knowledge, there has not been any report detailing the utilization of salt metathesis to selectively stain polyelectrolyte domains within a solid-state self-assembled block copolymer.…”

Section: Resultsmentioning

confidence: 99%

Multifunctional Block Copolymer: Where Polymetallic and Polyelectrolyte Blocks Meet

et al. 2015

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Sequential reversible addition−fragmentation transfer (RAFT) polymerization of a mixed sandwich cobaltocene monomer (η 5 -cyclopentadienyl-cobalt-η 4 -cyclobutadiene (CpCoCb)) and a phosphonium salt functionalized styrene monomer resulted in the first example of a unique multifunctional block copolymer consisting of a metallopolymer block and a polyelectrolyte block. The polyelectrolyte block was decorated with a gold anion (AuCl 4 − ) via salt metathesis, resulting in a heterobimetallic block copolymer with distinct gold and cobalt sections. Solution self-assembly behavior of this unique metallopolymer-b-polyelectrolyte copolymer before and after salt metathesis was studied. Heterobimetallic micelles with a gold containing core and a cobalt-containing corona were obtained, and then the core was reduced to form gold nanoparticles (AuNPs). Studies on the solid-state self-assembly of this unique block copolymer showed that it phase separated into hexagonally packed cylinders. Salt metathesis of the phase-separated block copolymers was utilized as the first example of a nonstandard selective staining method to exclusively stain the polyelectrolyte domains with the AuCl 4 − anion. Staining the metallopolymer domain by RuO 4 provided the complementary pattern. Pyrolysis of the self-assembled block copolymers resulted in magnetic cobalt-phosphate nanoparticles with 17% char yield.

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“…Some sample treatments such as selective staining or removal of one block can be used to enhance contrast. 56 Scanning electron microscopy or transmission electron microscopy examination of film cross sections allows for the characterization of the interior of film, but lack of contrast generally prevents direct imaging without staining or removal of one block. Another way to access 3D information is the "step by step" layer removal and surface imaging approach.…”

Section: Fundamental Considerationsmentioning

confidence: 99%

“…The same problem of distinction between the two blocks can be encountered in scanning electron microscopy, and charging effects can be problematic. Some sample treatments such as selective staining or removal of one block can be used to enhance contrast …”

Section: Fundamental Considerationsmentioning

confidence: 99%

Solvent Vapor Annealing of Block Polymer Thin Films

et al. 2013

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Synthesis of 2-Oxazolidinones. -The reaction of carbon dioxide with propargylic amines is promoted by a protic ionic liquid such as 1,8-diazabicyclo[5.4.0]-7-undecenium 2-methylimidazolide (DBM) that acts also as a solvent to give the corresponding oxazolidinones in high yields. The reaction proceeds under mild, metal-free conditions. The cheap and green solvent can be easily recycled and reused at least five times without significant loss of catalytic activity and selectivity. A reaction mechanism is proposed on the basis of detailed DFT studies. -(HU, J.; MA*, J.; ZHU, Q.; ZHANG, Z.; WU, C.; HAN, B.; Angew.

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Phase-selective staining of metal salt for scanning electron microscopy imaging of block copolymer film

Cited by 9 publications

References 28 publications

Solvent induced formation of an ordered nanorod array of gold/polymer composite by block copolymer film templating

Solvent induced formation of an ordered nanorod array of gold/polymer composite by block copolymer film templating

Multifunctional Block Copolymer: Where Polymetallic and Polyelectrolyte Blocks Meet

Solvent Vapor Annealing of Block Polymer Thin Films

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